DE102010047544A1 - Method for extracting of liquid helium from feed fraction containing helium, nitrogen and methane and/or oxygen in liquid helium trailer, involves subjecting nitrogen-containing fraction to cryogenic adsorptive cleaning process - Google Patents

Method for extracting of liquid helium from feed fraction containing helium, nitrogen and methane and/or oxygen in liquid helium trailer, involves subjecting nitrogen-containing fraction to cryogenic adsorptive cleaning process Download PDF

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DE102010047544A1
DE102010047544A1 DE201010047544 DE102010047544A DE102010047544A1 DE 102010047544 A1 DE102010047544 A1 DE 102010047544A1 DE 201010047544 DE201010047544 DE 201010047544 DE 102010047544 A DE102010047544 A DE 102010047544A DE 102010047544 A1 DE102010047544 A1 DE 102010047544A1
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nitrogen
helium
fraction
liquid helium
adsorptive
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Kirkor Kurtcuoglu
Ulrich Lindemann
Klaus Ohlig
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Linde GmbH
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Linde GmbH
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/0002—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the fluid to be liquefied
    • F25J1/0005—Light or noble gases
    • F25J1/0007—Helium
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/006—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the refrigerant fluid used
    • F25J1/007—Primary atmospheric gases, mixtures thereof
    • F25J1/0072—Nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/02—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process
    • F25J1/0221—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process using the cold stored in an external cryogenic component in an open refrigeration loop
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/02—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process
    • F25J1/0243—Start-up or control of the process; Details of the apparatus used; Details of the refrigerant compression system used
    • F25J1/0244—Operation; Control and regulation; Instrumentation
    • F25J1/0245—Different modes, i.e. 'runs', of operation; Process control
    • F25J1/0249—Controlling refrigerant inventory, i.e. composition or quantity
    • F25J1/025—Details related to the refrigerant production or treatment, e.g. make-up supply from feed gas itself
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/02—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process
    • F25J1/0243—Start-up or control of the process; Details of the apparatus used; Details of the refrigerant compression system used
    • F25J1/0257—Construction and layout of liquefaction equipments, e.g. valves, machines
    • F25J1/0261—Details of cold box insulation, housing and internal structure
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/02—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process
    • F25J1/0243—Start-up or control of the process; Details of the apparatus used; Details of the refrigerant compression system used
    • F25J1/0257—Construction and layout of liquefaction equipments, e.g. valves, machines
    • F25J1/0274—Retrofitting or revamping of an existing liquefaction unit
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0204—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the feed stream
    • F25J3/0209—Natural gas or substitute natural gas
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
    • F25J3/0257—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
    • F25J3/028—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of noble gases
    • F25J3/029—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of noble gases of helium
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/08—Separating gaseous impurities from gases or gaseous mixtures or from liquefied gases or liquefied gaseous mixtures
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/40—Processes or apparatus using other separation and/or other processing means using hybrid system, i.e. combining cryogenic and non-cryogenic separation techniques
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/60—Processes or apparatus using other separation and/or other processing means using adsorption on solid adsorbents, e.g. by temperature-swing adsorption [TSA] at the hot or cold end
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/42—Nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/30—Helium
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/42—Nitrogen or special cases, e.g. multiple or low purity N2
    • F25J2215/44—Ultra high purity nitrogen, i.e. generally less than 1 ppb impurities
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2220/00—Processes or apparatus involving steps for the removal of impurities
    • F25J2220/02—Separating impurities in general from the feed stream
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2220/00—Processes or apparatus involving steps for the removal of impurities
    • F25J2220/04—Separating impurities in general from the product stream
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/90—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration
    • F25J2270/904—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration by liquid or gaseous cryogen in an open loop
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2290/00—Other details not covered by groups F25J2200/00 - F25J2280/00
    • F25J2290/62—Details of storing a fluid in a tank

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  • Mechanical Engineering (AREA)
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Abstract

The method involves performing compression (A) of a feed fraction (1) and subjecting to nitrogen separation (B). A nitrogen-containing fraction (5) is split by nitrogen separation and subjected to a cryogenic adsorptive cleaning process (E). The cryogenic adsorptive cleaning process is adapted in such a manner that the nitrogen-containing fraction is cooled and adsorptive product is purified at a temperature of less than 80 K. The purification of the nitrogen-containing fraction is realized by a pressure swing adsorption, vacuum pressure swing adsorption and/or thermal swing adsorption.

Description

Die Erfindung betrifft ein Verfahren zum Gewinnen von flüssigem Helium aus einer wenigstens Helium, Stickstoff und Methan und/oder Sauerstoff enthaltenden Einsatzfraktion, wobei die Einsatzfraktion verdichtet, einer Stickstoff-Abtrennung unterworfen und anschließend verflüssigt wird.The invention relates to a process for recovering liquid helium from a feed fraction containing at least helium, nitrogen and methane and / or oxygen, wherein the feed fraction is compressed, subjected to a nitrogen removal and then liquefied.

Gattungsgemäße Verfahren zum Gewinnen von flüssigem Helium kommen in Heliumreinigungs- bzw. Heliumgewinnungsanlagen zur Anwendung. Die vorgenannte Einsatzfraktion stammt üblicherweise aus einer Erdgasquelle, weswegen neben Helium und Stickstoff auch Methan sowie ggf. Sauerstoff in der zu verflüssigenden Einsatzfraktion enthalten sind.Generic processes for obtaining liquid helium are used in helium purification or helium recovery plants. The aforementioned feed fraction usually originates from a natural gas source, which is why, in addition to helium and nitrogen, methane and possibly oxygen are also contained in the feed fraction to be liquefied.

Aus der Einsatzfraktion werden mittels thermischer Separation bzw. Rektifikation große Mengen Stickstoff abgeschieden. Dieser Stickstoff wird innerhalb des gattungsgemäßen Gewinnungsverfahrens an verschiedenen Stellen als Kühlmedium verwendet. Er wird dazu in einer Stickstoff-Verflüssigungsanlage auf eine Temperatur von ca. 80 K abgekühlt sowie verflüssigt und anschließend über ein Verteilsystem unterschiedlichen Stellen der Helium-Reinigungs- und -Verflüssigungsanlage zugeführt.From the feed fraction large amounts of nitrogen are separated by thermal separation or rectification. This nitrogen is used at various points as a cooling medium within the generic recovery process. It is cooled in a nitrogen liquefaction plant to a temperature of about 80 K and liquefied and then fed via a distribution system to different points of the helium cleaning and liquefaction plant.

Das mittels des gattungsgemäßen Verfahrens gewonnene flüssige Helium wird nach seiner Verflüssigung im Regelfall in geeigneten Speichervorrichtungen, beispielsweise Dewar-Behältern, zwischengespeichert und/oder mittels mobiler Flüssighelium-Trailer zum Ort seiner Verwendung transportiert. Der in dem gattungsgemäßen Verfahren zum Gewinnen von flüssigem Helium abgetrennte und verflüssigte Stickstoff (LIN) wird üblicherweise auch zur Kühlung der Strahlungsschilde der vorgenannten Helium-Speichervorrichtungen sowie Flüssighelium-Trailer genutzt.After its liquefaction, the liquid helium obtained by the generic method is as a rule temporarily stored in suitable storage devices, for example dewar containers, and / or transported to the place of use by means of mobile liquid helium trailers. The in the generic method for recovering liquid helium separated and liquefied nitrogen (LIN) is usually also used to cool the radiation shields of the aforementioned helium storage devices and liquid helium trailers.

Der im Zuge des Gewinnungsverfahrens aus der Einsatzfraktion abgeschiedene Stickstoff ist jedoch nicht rein, da er im Regelfall zumindest Methan und ggf. Sauerstoff enthält. Wird Methan- und/oder Sauerstoff-haltiger flüssiger Stickstoff in einem strömungsfreien Flüssigkeitsbad langsam verdampft, kommt es aufgrund der unterschiedlichen Verdampfungstemperaturen der einzelnen Komponenten zu einer Anreicherung von Methan und/oder Sauerstoff. Dies führt zur Bildung einer explosiven Atmosphäre.The separated in the course of the recovery process from the feed fraction nitrogen is not pure, since it usually contains at least methane and possibly oxygen. If methane and / or oxygen-containing liquid nitrogen is slowly evaporated in a flow-free liquid bath, enrichment of methane and / or oxygen occurs due to the different evaporation temperatures of the individual components. This leads to the formation of an explosive atmosphere.

Bei dem mit flüssigem Stickstoff gekühlten Strahlungsschild(en) von Flüssighelium-Trailern findet eine Verdampfung des flüssigen Stickstoffs aus einem Flüssigkeitsbad heraus statt. Derartige Flüssighelium-Trailer sind u. U. über einen längeren Zeitraum unterwegs. Während dieses Zeitraumes kann die Flüssigkeitsverdampfung und damit die Stoffzusammensetzung in dem LIN-gekühlten Strahlungsschild nicht kontrolliert werden. Es muss daher gewährleistet sein, dass Komponenten, von denen möglicherweise eine Gefahr ausgeht, nicht mit dem als Kühlmedium benötigten Stickstoff in den Flüssighelium-Trailer gelangen können.In the case of the liquid nitrogen radiation shield (s) of liquid helium trailers, liquid nitrogen evaporates from a liquid bath. Such liquid helium trailers are u. U. on the road for a long period. During this period, the liquid evaporation and hence the composition of matter in the LIN-cooled radiation shield can not be controlled. It must therefore be ensured that components which could possibly pose a hazard can not reach the liquid helium trailer with the nitrogen required as cooling medium.

Aufgabe der vorliegenden Erfindung ist es, ein gattungsgemäßes Verfahren zum Gewinnen von flüssigem Helium anzugeben, das neben der Gewinnung von flüssigem Helium die Gewinnung von hochreinem flüssigem Stickstoff ermöglicht.Object of the present invention is to provide a generic method for recovering liquid helium, which in addition to the recovery of liquid helium allows the recovery of high-purity liquid nitrogen.

Zur Lösung dieser Aufgabe wird ein Verfahren zum Gewinnen von flüssigem Helium vorgeschlagen, das dadurch gekennzeichnet ist, dass die mittels der Stickstoff-Abtrennung gewonnene Stickstoff-enthaltende Fraktion einem kryoadsorptiven Reinigungsprozess unterworfen wird.To solve this problem, a method for recovering liquid helium is proposed, which is characterized in that the nitrogen-containing fraction obtained by means of the nitrogen removal is subjected to a cryo-adsorptive purification process.

Weitere vorteilhafte Ausgestaltungen des erfindungsgemäßen Verfahrens zum Gewinnen von flüssigem Helium sind dadurch gekennzeichnet, dass

  • der kryoadsorptive Reinigungsprozess derart ausgelegt ist, dass die Stickstoffenthaltende Fraktion zunächst auf eine Temperatur von weniger als 100 K, vorzugsweise weniger als 80 K abgekühlt und anschließend adsorptiv gereinigt wird,
  • – die adsorptive Reinigung der abgekühlten, Stickstoff-enthaltenden Fraktion mittels eines PSA-, VPSA- und/oder TSA-Prozesses realisiert wird, und
  • – sofern das gewonnene flüssige Helium zumindest teilweise einem Helium-Speicher, vorzugsweise einem Flüssighelium-Trailer zugeführt wird und der oder die verwendeten Helium-Speichervorrichtungen mittels Stickstoff gekühlt werden, zumindest ein Teilstrom der in dem kryoadsorptiven Reinigungsprozess gewonnenen hochreinen Stickstoff-Fraktion zur Kühlung des oder der Helium-Speichervorrichtungen verwendet wird.
Further advantageous embodiments of the method according to the invention for obtaining liquid helium are characterized in that
  • the cryo-adsorptive purification process is designed such that the nitrogen-containing fraction is first cooled to a temperature of less than 100 K, preferably less than 80 K and then purified by adsorption,
  • - The adsorptive purification of the cooled, nitrogen-containing fraction is realized by means of a PSA, VPSA and / or TSA process, and
  • - If the recovered liquid helium is at least partially supplied to a helium storage, preferably a liquid helium trailer and the helium storage devices used or are cooled by nitrogen, at least a partial stream of the obtained in the kryoadsorptiven cleaning process high-purity nitrogen fraction for cooling the or the helium storage devices is used.

Das erfindungsgemäße Verfahren zum Gewinnen von flüssigem Helium sowie weitere vorteilhafte Ausgestaltungen desselben seien nachfolgend anhand des in der Figur in schematisierter Form dargestellten Helium-Verflüssigungsprozesses näher erläutert.The inventive method for obtaining liquid helium and further advantageous embodiments thereof are explained in more detail below with reference to the helium liquefaction process shown in schematic form in the figure.

Bei diesem wird eine wenigstens Helium, Stickstoff sowie Methan und/oder Sauerstoff enthaltende Einsatzfraktion über Leitung 1 einer Verdichtungseinheit A zugeführt. In dieser wird die Einsatzfraktion vorzugsweise mehrstufig auf einen Druck zwischen 10 und 40 bar verdichtet. Die verdichtete Einsatzfraktion wird anschließend über Leitung 2 einer Stickstoff-Abtrennungseinheit B zugeführt. Die über Leitung 3 aus der Stickstoff-Abtrennung B abgezogene Helium-Fraktion wird anschließend in einer Verflüssigungseinheit C verflüssigt. Das verflüssigte Heliumprodukt wird über Leitung 4 einem Flüssighelium-Trailer D zugeführt und in diesem zu seinem Bestimmungsort transportiert.In this case, an at least helium, nitrogen and methane and / or oxygen-containing feed fraction via line 1 a compression unit A is supplied. In this, the feed fraction is preferably compressed in several stages to a pressure between 10 and 40 bar. The compressed feed fraction is then transferred via line 2 a nitrogen separation unit B supplied. The over line 3 The helium fraction withdrawn from the nitrogen separation B is subsequently liquefied in a liquefaction unit C. The liquefied helium product is sent via pipe 4 fed to a liquid elite trailer D and transported in this to its destination.

In der vorerwähnten Stickstoff-Abtrennungseinheit B wird im Regelfall rektifikatorisch eine Stickstoff-reiche Fraktion aus der verdichteten Einsatzfraktion 2 abgetrennt. Diese Stickstoff-reiche Fraktion wird nunmehr über Leitung 5 einem erfindungsgemäß vorzusehenden kryoadsorptiven Reinigungsprozess E zugeführt. In diesem wird die Stickstoff-reiche Fraktion zunächst auf eine Temperatur von weniger als 100 K, vorzugsweise weniger als 80 K abgekühlt und anschließend adsorptiv gereinigt wird, Die adsorptive Reinigung der abgekühlten, Stickstoff-reichen Fraktion erfolgt hierbei mittels eines PSA-, VPSA- und/oder TSA-Prozesses, der derart auszulegen ist, dass er Methan und/oder Sauerstoff aus der Stickstoff-reichen Fraktion abzutrennen vermag.In the aforementioned nitrogen separation unit B, a nitrogen-rich fraction from the compressed feed fraction is usually rectificatively 2 separated. This nitrogen-rich fraction is now over line 5 an inventively provided cryo-adsorptive cleaning process E supplied. In this, the nitrogen-rich fraction is first cooled to a temperature of less than 100 K, preferably less than 80 K and then adsorptively cleaned, the adsorptive purification of the cooled, nitrogen-rich fraction is carried out by means of a PSA, VPSA and / or TSA process, which is to be designed so that it can separate methane and / or oxygen from the nitrogen-rich fraction.

Aus dem kryoadsorptiven Reinigungsprozess E wird über Leitung 6 eine hochreine Stickstoff-Fraktion abgezogen und einem Verflüssigungsprozess F unterworfen. Wie bereits eingangs erwähnt, wird der verflüssigte Stickstoff zumindest teilweise als Kühlmedium innerhalb des vorbeschriebenen Verfahrens zum Gewinnen von flüssigem Helium verwendet. In der Figur ist dies durch die Leitungen 7 und 8 dargestellt, über die verflüssigter Stickstoff der Stickstoff-Abtrennungseinheit B sowie der Heliumverflüssigungseinheit C zugeführt wird:
Bei der Verwendung des hochreinen Stickstoffs als Kühlmedium für die Strahlungsschilde von Helium-Speichervorrichtungen, insbesondere in Flüssighelium-Trailern, ist nunmehr sichergestellt, dass es nicht zur Anreicherung von gefährlichen Komponenten kommen und somit eine Explosionsgefahr wirkungsvoll verhindert werden kann.From the cryo-adsorptive purification process E is via line 6 withdrawn a high purity nitrogen fraction and subjected to a liquefaction process F. As already mentioned, the liquefied nitrogen is at least partially used as a cooling medium within the method described above for the recovery of liquid helium. In the figure, this is through the wires 7 and 8th via which liquefied nitrogen is fed to the nitrogen separation unit B and to the helium liquefaction unit C:
When using the high-purity nitrogen as a cooling medium for the radiation shields of helium storage devices, especially in liquid helium trailers, it is now ensured that it does not come to the accumulation of hazardous components and thus an explosion hazard can be effectively prevented.

Darüber hinaus kann der verflüssigte Stickstoff über Leitung 9 dem erwähnten Flüssighelium-Trailer D als Kühlmittel für dessen Strahlungsschild(e) zugeführt werden.In addition, the liquefied nitrogen over line 9 the mentioned liquid helium trailer D as a coolant for the radiation shield (s) are supplied.

Die Verwendung von hochreinem Stickstoff, der mittels des erfindungsgemäß vorzusehenden kryoadsorptiven Reinigungsprozesses gewonnen wird, als Kühlmedium innerhalb des Helium-Verflüssigungsprozesses hat nunmehr den Vorteil, dass der Verbrauch an Kühlmedium verringert werden kann, da durch die Abwesenheit unerwünschter Komponenten im Kühlmedium die unerwünschte Verschiebung des Siedepunktes vermieden werden kann.The use of high-purity nitrogen, which is obtained by means of the present invention to be provided cryo-adsorptive cleaning process as a cooling medium within the helium liquefaction process now has the advantage that the consumption of cooling medium can be reduced, since the unwanted shift in the boiling point due to the absence of undesirable components in the cooling medium can be avoided.

Der kryoadsorptive Reinigungsprozess für die aus der wenigstens Helium, Stickstoff sowie Methan und/oder Sauerstoff enthaltenden Einsatzfraktion abgetrennten Stickstoff-reichen Fraktion kann bei bestehenden Helium-Verflüssigungsprozessen problemlos und mit einem vergleichbar geringem Aufwand nachgerüstet werden, da der eigentliche Verflüssigungsprozess dabei unverändert bleibt.The cryo-adsorptive purification process for the nitrogen-rich fraction separated from the feed fraction containing at least helium, nitrogen and methane and / or oxygen can be easily retrofitted to existing helium liquefaction processes with comparatively little effort since the actual liquefaction process remains unchanged.

Claims (4)

Verfahren zum Gewinnen von flüssigem Helium (4) aus einer wenigstens Helium, Stickstoff und Methan und/oder Sauerstoff enthaltenden Einsatzfraktion (1), wobei die Einsatzfraktion (1) verdichtet (A), einer Stickstoff-Abtrennung (B) unterworfen und anschließend verflüssigt wird (C), dadurch gekennzeichnet, dass die mittels der Stickstoff-Abtrennung (B) gewonnene Stickstoff-enthaltende Fraktion (5) einem kryoadsorptiven Reinigungsprozess (E) unterworfen wird.Process for recovering liquid helium ( 4 ) from an at least helium, nitrogen and methane and / or oxygen-containing feed fraction ( 1 ), the feed fraction ( 1 ) is compressed (A), subjected to a nitrogen removal (B) and then liquefied (C), characterized in that the nitrogen-containing fraction (N) obtained by means of the nitrogen removal (B) 5 ) is subjected to a cryo-adsorptive cleaning process (E). Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass der kryoadsorptive Reinigungsprozess (E) derart ausgelegt ist, dass die Stickstoff-enthaltende Fraktion (5) zunächst auf eine Temperatur von weniger als 100 K, vorzugsweise weniger als 80 K abgekühlt und anschließend adsorptiv gereinigt wird.A method according to claim 1, characterized in that the cryo-adsorptive purification process (E) is designed such that the nitrogen-containing fraction ( 5 ) is first cooled to a temperature of less than 100 K, preferably less than 80 K and then purified by adsorption. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass die adsorptive Reinigung der abgekühlten, Stickstoff-enthaltenden Fraktion mittels eines PSA-, VPSA- und/oder TSA-Prozesses realisiert wird.A method according to claim 1 or 2, characterized in that the adsorptive purification of the cooled, nitrogen-containing fraction by means of a PSA, VPSA and / or TSA process is realized. Verfahren nach einem der vorhergehenden Ansprüche 1 bis 3, wobei das gewonnene flüssige Helium (4) zumindest teilweise einem Helium-Speicher, vorzugsweise einem Flüssighelium-Trailer (D) zugeführt wird und der oder die verwendeten Helium-Speichervorrichtungen mittels Stickstoff gekühlt werden, dadurch gekennzeichnet, dass zumindest ein Teilstrom der in dem kryoadsorptiven Reinigungsprozess (E) gewonnenen hochreinen Stickstoff-Fraktion (9) zur Kühlung des oder der Helium-Speichervorrichtungen verwendet wird.Method according to one of the preceding claims 1 to 3, wherein the recovered liquid helium ( 4 ) is at least partially supplied to a helium reservoir, preferably a liquid helium trailer (D), and the helium storage device or devices used are cooled by means of nitrogen, characterized in that at least a partial flow of the high-purity nitrogen recovered in the cryo-adsorptive purification process (E) Fraction ( 9 ) is used to cool the helium storage device (s).
DE201010047544 2010-10-05 2010-10-05 Method for extracting of liquid helium from feed fraction containing helium, nitrogen and methane and/or oxygen in liquid helium trailer, involves subjecting nitrogen-containing fraction to cryogenic adsorptive cleaning process Withdrawn DE102010047544A1 (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105987580A (en) * 2016-02-03 2016-10-05 安徽万瑞冷电科技有限公司 Neon and helium rare gas separating and refining process method with refrigerator as cold source
CN111288748A (en) * 2019-10-11 2020-06-16 中国人民解放军63810部队 Helium purification device and helium purification method

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105987580A (en) * 2016-02-03 2016-10-05 安徽万瑞冷电科技有限公司 Neon and helium rare gas separating and refining process method with refrigerator as cold source
CN111288748A (en) * 2019-10-11 2020-06-16 中国人民解放军63810部队 Helium purification device and helium purification method

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